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Determination of trace impurity elements in high purity indium through glow discharge mass spectrometry method

A trace impurity, high-purity technology, applied in measuring devices, material analysis through electromagnetic means, instruments, etc., can solve the problems of cumbersome operation, long process, easy introduction of contamination, etc.

Inactive Publication Date: 2014-06-25
GENERAL RESEARCH INSTITUTE FOR NONFERROUS METALS BEIJNG
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Problems solved by technology

[0002] At present, the determination methods of trace impurity elements in high-purity indium include chemical methods (silver diethylaminodithiocarbamate (Ag-DDC) method, silicon molybdenum blue absorptiometry, hydroiodic acid, sodium hypophosphite reduction polarography etc.) These methods are cumbersome and difficult to master
In addition, there are chemical spectroscopy and graphite furnace atomic absorption methods for the determination of trace impurities in high-purity indium. This method has a long process and is easy to introduce contamination.

Method used

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  • Determination of trace impurity elements in high purity indium through glow discharge mass spectrometry method

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Embodiment Construction

[0019] Sample pre-sputtering: put the sample into the sample holder, push it into the ion source cavity, wait until the vacuum reaches 2.2~2.4mbar, adjust the discharge voltage and discharge current to 0.9~1.2kV, 40~45mA, and sputter about 30 ~40min, generally based on the stable signals of Na, Fe and Ca, which are easy to introduce contamination, to eliminate possible contamination during sample preparation.

[0020] Quantitative determination: adjust the discharge voltage to 0.9-1.2kV, discharge current to 40-45mA, carry out high-voltage discharge, collect ion signals of the elements to be measured, and calculate the concentration of impurity elements to be measured according to the quantitative analysis principle of the glow discharge mass spectrometer. Table 1 shows the measurement results of high-purity indium (≥6N).

[0021] Table 1 Experimental results

[0022]

[0023] .

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Abstract

The invention relates to a determination method for trace impurities in a rare metal, particularly to a determination method for trace impurities in high purity indium. The determination method comprises: (1) cutting a sample into a sheet, washing oil stain on the sample surface with toluene, washing with ultrapure water, etching for 8 min with 50% (volume concentration) nitric acid, repeatedly rinsing with ultrapure water, storing in methanol, and taking and drying under an infrared lamp before analysis; (2) placing the sample in a sample clamper, pushing into an ion source chamber, respectively adjusting the discharge voltage and the discharge current to 0.9-1.2 kV and 40-45 mA when the vacuum degree achieves 2.2-2.4 mbar, and sputtering for about 30-40 min, wherein generally stabilization of signals of Na, Fe and Ca easily introducing contamination is adopted as the reference so as to eliminate possibly-produced contamination during the sample preparation process; and (3) respectively adjusting the discharge voltage and the discharge current to 0.9-1.2 kV and 40-45 mA, carrying out high voltage discharge, collecting the ion signals of the elements to be detected, and calculating the concentration of the impurity elements to be detected according to the quantitative analysis principle of the glow discharge mass spectrometer. The method has characteristics of simple operation, less interference and short process, and can well meet requirements of determination of trace impurities in high purity indium.

Description

technical field [0001] The invention relates to a method for determining trace impurity elements in rare metals, in particular to a method for determining trace impurities in high-purity indium. Background technique [0002] At present, the determination methods of trace impurity elements in high-purity indium include chemical methods (silver diethylaminodithiocarbamate (Ag-DDC) method, silicon molybdenum blue absorptiometry, hydroiodic acid, sodium hypophosphite reduction polarography etc.) These methods are cumbersome to operate and difficult to master. In addition, there are chemical spectroscopy and graphite furnace atomic absorption methods for the determination of trace impurities in high-purity indium. This method has a long process and is easy to introduce contamination. Therefore, it is necessary to develop a simple and feasible method that can satisfy the determination of trace impurities in high-purity indium (≥6N). Contents of the invention [0003] The purpo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/68
Inventor 刘红李爱嫦
Owner GENERAL RESEARCH INSTITUTE FOR NONFERROUS METALS BEIJNG
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